Detection of Florfenicol Residues in Salmon Trout via GC-MS

A reliable and sensitive method based on solid-phase extraction was developed for the simultaneous detection of florfenicol (FF) and its metabolite florfenicol amine (FFA) in market fish samples. Fish samples were extracted with ethyl acetate. Lipids were removed from the extracts using hexane, followed by cleaning via solid-phase extraction and derivatization with BSTFA + TMCS [(N,O-bis (trimethylsilyl) trifluoroacetamide) + trimethylchlorosiane, (99:1)]; the fish samples then underwent gas chromatography with electron impact ionization mass spectrometric detection in the selected ion-monitoring mode, using 1 target and 3 qualifier ions. The method was validated according to EU Commission Decision 2002/657/EC. Mean recovery ranged from 84.09 to 100.9 %, with a coefficient of variation < 2.7 when samples were spiked at 3 different concentrations. The decision limits and detection capability of the method were 534 and 585 mu g kg(-1) for FF and 541 and 602 mu g kg(-1) for FFA, respectively. This validated method was successfully applied for the analysis of FF and FFA residues in fish samples obtained from local markets in Turkey.